DE1769654A1 - Polymer molding compound - Google Patents

Description

The invention relates to a Polyraer Pormmasse on Ba- * than of high pressure polyethylene, the improved processability has, and relates in particular to such a polymer Pormmai ne, the next to ilochdtiickpolyavhylun ataktlsches polypropylene or contains an atactic ethylene-propylene copolymer and for TxUf high-performance machines.

Due to its excellent properties, polyethylene is used in numerous areas of application for molded bodies, ¥ / ie beie Ftlme, PoIi ^ n, Pipes and Fibers, and also as

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Electric wire covering material used. There are many Try to improve the properties of polyethylene even further to enhance. High-pressure polyethylene has a comparison to low-pressure polyethylene, polypropylene and other a-01efin polymers, obtained by medium-pressure or low-pressure polymerization processes have excellent properties. However, the high pressure polyethylene has no properties that it for processing on high-performance machines, which have been used in increasing numbers in recent years, can be processed do. The requirement of processability on high-performance machines has become more and more urgent. This is especially true for use as an insulating cover for electrical wires, whereby according to J.N. Scott, C.T. Levette, C.P. Leslie et al "Tailoring of High Density Polyethylene for High Speed Wire Coating "The 14th Wire & Cable Symposium, a processing speed of approx. 1500 m / min, is required. For this the processability and the melt flow properties exhibited by high pressure polyethylene are not lesser sufficient.

For improving workability, melt flow properties, general elongation resistance to break, and the like physical properties of high pressure polyethylene are numerous efforts have already been made. For example, in Japanese Patent Publication No. 17410/1964, British Patent No. 1,032,728 and Dutch patent specification No. 6610590 describes processes, bsi which low pressure polyethylene in high pressure polyethylene is incorporated. Dutch patent specification no * 6610590 describes a method in which crystalline polypropylene is incorporated) In Japanese Patont Publication No. 22 351/1964 a method is disclosed in which a crystalline α-olefin polymer is incorporated! from Japanese Patent Publication No. 21 210/1963, the German patent specification No. 1 137 859 and the French »; Patent No. 1 452 469 processes are known in which

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a crystalline ethylene-propylene copolymer, a ethylene-propylene block copolymer or a crystalline copolymer of ethylene or propylene and an α-olefin with 4 or more carbon atoms is added to the high-pressure polyethylene; in Japanese Patent Vsröffontllchung no. 20 266/1965 $ British Patent Specification no. 1037820 and the Amari kanis around Pat. No. J> 261,889 are bsschrleben methods in which a Kthylen-propylene rubber, an ethylene-propylene "terpolymer or an ethylene-propylene-wax copolymer can be added? Japanese Patont Publication No. 14 625/1962 describes a method in which polypropylon wax is incorporated; British Patent No. 96O 311 describes a method in which polyisobutylene, polystyrene or the like is mixed with high pressure polyethylene and the mixture is heated and a process is also known in which two or more of the above-mentioned polymers are added and kneaded with the high-pressure polyethylene.

However, the process at dom has high-pressure polyethylene with Low pressure polyethylene, polypropylene or homopolymers or Copolyraeren of other a «0! © fines or with single crystalline ones Polymer, as a block copolymer is processed and forbidden, disadvantages as described below.

The low pressure polyethylene or a similar polymer used in High pressure polyethylene has a hühores Molecular weight than the high pressure polyethylene and has one thing poor in compatibility, and when considering the resultant Examination of the mixture microscopically after knotting shows that the polymer is not in the polyethylene evenly distributed. As a result, the mixture has low tensile strength and elongation and must be subjected to high extrusion pressure be extiuated.

On the other hand, the process at dsm is high pressure polyethylene

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with a rubbery copolymer of α-olefins, dao mainly is made of ethyl or propylene, is vorarboitot, to improve the general fracture-elongation resistance of high-thickness polyethylene is expedient. Dicso's procedure is but not satisfactory if the availability of high pressure polyethylene to be improved on high-performance machines. A »obtained according to the method described above Molding compound generally has a high viscosity and is not suitable for excellent behavior want to achieve. Even if the after the above The molding compound obtained in the process has a low viscosity, the molded bodies obtained by extrusion molding have no sufficiently smooth surface.

As mentioned above, the known methods are not sufficient to improve the processability of plasticised nylon on high-quality machines. Hit'dem Auedruck "Vorarböltbarkeit on HochJ.ßiatiuxgijraaschiniin ¹¹ is printed ^ nschaft in diosor description, a Eiß, it dio allows even at very Buckle ab3anfanden Wirfnhren as beißpifllsweisn bnira Aui'brlngen a j [shall" RLIB ^f irr, on ugs "Inen JSlßktrodraht, dor i>trani.; PreiJdru (;! (. Low and the oil surface of the product is very smooth, as in the usual process for the production of Forckurporn, such as films, foils, pipes and fibers from the company .fl is.

Quite generally ^ iii ^ in wiixi brdm Ubnrsiohon von Kloktrodriihten the one with a forramasn «? z \\ iibürsiclionde wire stretched otlirker with zundiimmdcra expressing pressure biiiin Entiuiioren the Fornniasso, wherein the DurclJir.ijss'U ¹ dor Drahtnesie is lcloiner and the wire core is wHhrend processing is cured. This creates such disadvantages that the tolerance for the subsequent winding and assembly stages is lower and the wire sometimes breaks accidentally.

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The invention is based on the object oine Polyraor-Forraraasse based on high pressure polyethylene to cohaffon, the Glno verbassorba preparable cold on high performance machine. The invention also relates to the method for Manufacture of such a Polywar porm mass.

This object is achieved by means of a Polymar-Pornamsse based on high pressure polyethylene, which is characterized in that it consists essentially of (1) 70 to 99 * 5 ll \ m .- # of high pressure polyethylene, since "a density of 0, 9 ^{ H) or less bulges, and (2) 0.5 to 30 Göw. ~ # (A) an essentially amorphous polypropylene, which is a moderately soluble polymurlsationa secondary product from the division of crystalline polypropylene with the use of an ous a titanium halogen and an aluminum alkyl consisting of a catalyst, (b) an essentially amorphous propylene-ethylene copolymer, which is used as a moderately insoluble polyamide ionic product for the production of crystalline propylene-methyl-ethylene-ethyl-methyl-ethylene-propylene polymer -Bloclccorjolyrasr, which consists essentially of propylene, with the wounding of a titanium halide and an aluminum alkyl carbonate catalyst, odor (ο) a mixture dlssos in the weekly morpho n polypropylene and this in the usually amorphous propylene-ethylene copolymer.

The high-pressure polyethylene, which is a component of the molding compound according to the invention, has a density of 0.9 * 10 or less, preferably 0.917 to 0.9 ^ 0, and a melt index of. 0.1 to 5.0, and is a homopolymer or copolymer of methylane / ethylene or at least 50% ethyl and the remainder is a comonomer, such as vinyl acetate or ethyl acrylate containing the mixture is polymerized in a tubular reactor or autoclave type <3n reactor at 50 to 300 ⁰ C under a pressure of 500 to 4000 atm in the presence of oxygen, organic peroxides or azo compounds as a catalyst.

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The further component of the molding composition according to the invention is a substantially hydrocarbon-soluble amorphous polypropylene and / or substantially hydrocarbon-soluble amorphous propylene-ethylene copolymer as defined below.

The amorphous polypropylene is an essentially hydrocarbon-soluble polymer which is produced by homopolymerization of propylene in an n-hydrocarbon solvent such as n-heptane as a solvent in the presence of a titanium halide such as, for example, 3 TiCl ^ 'AlCl ,, and an aluminum alkyl compound such as Al (ethyl) pCl, separating the suspended contaminants from the reaction product and recovering the polymer from the remaining hydrocarbon solution. This amorphous polypropylene has in tetralin at 135 ⁰ C a viscosity number £ V) _7 of 0.2 to 0.6 and a determined by conventional X-ray analysis of crystallinity of 35 parts by weight or less Ϊ. The amorphous ethylene-propylene copolymer is an essentially hydrocarbon-soluble copolymer which, when a crystalline ethylene-propylene copolymer or a crystalline ethylene-propylene block copolymer consisting essentially of propylene is obtained, by copolymerization of ethylene with propylene in an n- Hydrocarbon solvent in the presence of a titanium halide such as 3TiCl, 'AlCl ,, and an aluminum alkyl compound such as Al (ethyl) pCl, as a catalyst, separating the suspended contaminants from the reaction product and recovering the copolymer from the remaining hydrocarbon solution been received 1st. This amorphous copolymer is a copolymer with an ethylene content of 20% by weight or less, a viscosity number C ^) J in tetralin at 135 ⁰ C of 0.2 to 2.8, preferably 1.0 to 2.8 and a crystallinity of 35% by weight * or less, determined by means of conventional X-ray analysis. The two substances, the essentially hydrocarbon-soluble amorphous polypropylene and the amorphous propylene-ethylene copolymer, can be used in the molding composition according to the invention. The amorphous propylene-ethylene copolymer is preferably used . It is

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it is also possible to use the essentially carbon detoxification material amorphous polypropylene and the era essential; borrowed icöhlcawaßEiö soluble amorphous propylene-nylon copoi'iner cleichaöitiß see below use.

It found \ n \ VDQ that dlc3ae by incorporating amorphous polypropylene which tinter as Nobenprodukt in naratoXlimß crystalline polypropylene using a from Oins; obtained bastohcnden n Tltanhnlögentd and Elnor AXitininimnalkrl-VerbJjidimß catalyst, or the amorphous Propylon-Kthylen-Oopolymers, that as iTobcnprcäulct bai der H'srtstolluns cin <53 Icrirstalllnen Kthyl ^ n-Propylcn-Ccpolynssrs or a! criatnllinen rropylen-Kthylt ^ i '-'Blockcopoli'Körs under Venfßnclims eloUtho. rarity of Kochdrucl ^ olyilthylena on Hochlclclstußssnaschiiiön can be improved.

The orfinöimsßgGinaße Pormaaase aöigt one Customized "rs EUSS (s <3seiciinete Verarb3itfcsrkoit on !! ochJ.aiotvjatßnraasoiilirm, \ t & m sio by adding from 0.3 to 30 Gsw.-jS this aisorphiui PolypropyÜcns or dioseo anorphon propylene»? ^(R fcb5 LCN Coro3.yra ^r irs ζλλ ΗοοΜηχοΙί «polyethylene Höro3tellt 1st. Insb ^ rjondore then, wcam dia additional nKsneo 1 bit 10 GiiW.«> Ji amounts, orhltlt inoii ß ^ .ns Foni- '. Jaöce, which is expressed at niodrigo ^ osa dian and results in smooth surfaces.

If you think of the inventive Pormssasse as XcolicrUbarzug for Elelrtrowires want to end, it is advantageous to work in this way, that, according to the Uborziohsn, the form dimensions are so by application organic peroayds or elolctron rays and at the same time the surface is hardened. Especially when you use the amorphous polypropylon or the amorphous propylene-ethylene copoly « ever added in large quantities, you can mäfien Pormmasse auagezoiebnete Eißennchaftwa

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When preparing the molding composition according to the invention, one can the individual components using any known method each other, for example using a Banbury mixer, a roller kneader, or a screw extruder.

The inventive polymer molding material can be used for numerous Application zvjeclce are used. You can do this as with known Polymers suitable hang of various common stabilizers, "Copper initiators, fillers, reinforcing agents, Karze or - / taf blowing agents and coloring agents, such as Pigments.

As said, the present invention improves the processability dös of polyethylene on heavy duty machines has been improved · It is now possible, for example, under Use of Poraiaasse polyethylene coatings according to the invention Manufacture of electrical wires with high speed UuÖorst *

Invention geinäö was also for so far as by-products Accruing substances created a good possibility of use, d'.inn amorphous polypropylene or amorphous © Propylene-Kthylan-Copolj / iner, which in the inventiongeniUßen molding material are, as already mentioned, by-products of the production of crystalline polypropylene, crystalline propylene "KthyiGn-CcpGlyt3 © r. cdar crystalline propylene-ethylene block copolymer, which mainly consist of propylene.

In the examples below, some of the methods used with the USon Molding compound achievable in detail illustrated. In each of the examples, the processability the Polymer ^ ForaimassG under very severe conditions, they wlo are listed below.

A spray head with a diameter of 0.6 can was inserted into a Schneokenstrungsprung with οinum diameter of 30 mm and one

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Ratio of effective length to effective diameter of 20 used. A polymer porous mass was extracted from the screw extruder and a copper wire with a diameter of 0 _sec . The processability of the molding compound was estimated using various measuring methods, for example the pressure occurring inside the spray head when the molding compound was extruded from the Schneeken extrusion press was measured * the surface of the overmolded wire was assessed visually and by scanning! the surface roughness measurement device (manufactured by Tokyo Selmitsu ICK.) was found to have smoothness of the face! and the surface was observed optically by means of a microscope at a magnification of 300 times. In addition, the physical properties of the polyamide molding compound were determined by measuring technology after the wire had been overmolded, after the wire core had been pulled out of the overmolded electrical wire.

The physical properties of the molding compositions illustrated in the B313spielön were determined by means of customary methods. For example, the Schmölsindöx; according to the American standard ASTM D I283-57 T, the density by measuring the density-oil gradient in one meter (at 20 ⁰ C), the viscosity number fo] in l'etralin jriisung at 135 ⁰ C, and the ethylene concentration in the copolymer determined by means of infrared spectrophotometric

All percentages mean oil percentages. The elongation was determined in accordance with JIS K 6? 61 - 1962. The condition of the coated surface was divided into degrees of quality such that the evaluation determined by touch and the result of the measurement by means of the device for determining the surface roughness were evaluated together and the best surface condition with 1, the worst

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Surface condition was set at 10. The abrasion resistance was best icon t that a defined weight attached to one end of the overmolded wire and placed the wire on a horizontal drum made of metal, and through Rotleren the drum has been subjected to abrasion. The value for the abrasion resistance was given by the number of revolutions of the drum until the spray coating broke were carried out.

example 1

As a component of high-pressure polyethylene has been g having a melt index of 0.22 / 10 min, and as the other component in a hot n-heptane-soluble ethylene copolymer Propylon (CHT ^"2 * 5 * Kthylengehalt: 15 #)., Which at a the production of a crystalline polymer in an n-heptane solvent in the presence of a 3TiCl ₃ ⁰ AlCl ₅ - Al (ethyl) ₂ Cl catalyst system (With 8'J *? polypropylene chain "fan the block copolytp.aren was accrued by-product. The last-mentioned component was 0.1 % of 1,1,3-tris (2-methyl-5-tert-butyl-4-hydro3cyphenyl) -butane has been incorporated. the two components were placed in the juigögebenen in Table Ϊ proportionate manganese in a 0-type Banbury mixer, and 7 minutes knotted together at 135 ⁰ C. After kneading, the resulting mass was pelletized in a conventional pelletizer Then became di e granulated mass is introduced into the aforementioned screw extruder and tested for its behavior when overmoulding a copper wire at high linear speed. The results are illustrated / polymerized in Table I,

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Table X

attempt
Kr. Poly
ethylene in hot n-Hsptane
soluble ethylene
Propylön-Gopoljnner Squeeze
pressure: _o
(kß / cnr) Surface
roughness ¹
2
3
4th
5
6th 100
99.5
99.0
97.0
90.0
80.0 0
0.5
i »0
3.0
10.0
20.0 396
■: 385
380
378
351
310 10
5
3
2
1
1

Example 2

As a component, high pressure polyethylene was used with a Schm3lzinde3t of 0.20 g / 10 Kin- and a density of 0.930 are used. The other component was one in hot n-keptane Soluble ethylene ~ propylene-n «copolymer ([Vj]« 0.5 * ethylene content: 10 £>) used. This was a by-product of the all in one n-heptane solvent in the presence of a 3TiCl ^ 'AlCl,

Al (ethyl) ₂ Cl-Kataly3atorEtfTiten! S carried out the production of a statistical ethylene-propylene-Ccpolymer (ethylene content 3 %) » which was insoluble in heptane owing to the isotalctic structure of the propylene chain. The two components were kneaded with one another as described in Example 1, and the resulting mass was subjected to the injection molding tests. The results are shown in Table II.

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- 12 - Table II

attempt
JJr. 2> usatmi! SsnsGtzun3 (Geif .- #) in hot n-heptar
soluble Kthylc-n-
PropjrXen-CopoXymsi Squeezing
druel: _n Surfaces"
roughness 7th
8th Poly
ethylene 0 410 10 100
97.0

Example 3

High-pressure polyethylene with a Schraals index of 0.25 g / 10 min and a density of 0.920 was used as the oliva component. As <2io endor «? The component was made into n-heptane-soluble atalctic polypropylene (Ji3 ^ 0.8) eioßetat, which was obtained from an n-heptiine-Sohicht SG, which was entetojidcn in the manufacture of Iosofcactic in polypropylene, if IVopylea in antiquity 3? ICL, 'AlCl _.-AlClltliyl) ₀ Cl-Katalycatoreyetcras Sxi an n-Käptün-LücnngGralttol tcsopolyraerisiert and subsequently a in n ~ Hoptan ~ insoluble polynior was separated off. The two components were letted together as in Eoicpiel 1 baechrioban, and the resulting cash register was subjected to fuel testing. The results are shown in Table III.

Table III

Try
ir. Poly
ethylene in n-heptane loess
liohss atactic
Propylon Polyraar Express
drucic ρ
(kr / cm) Surfaces-
roughness 9
10 100
97 0
5.0 390
5 ^ 0 9
4th

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As a component mtrde high pressure polyethylene with a Binolzindex of 0.2 ^ g / 10 Kin. and a density of 0.924 used. When the other component became one in hell n-heptane ~ soluble ethylene-propylene copolymer (f *) l «2.2j KthylengGhalts $ 8) is used. It was about one in an n-Hsptane solvent in the presence of a ^ TiCl ^ 'AlCl -. ^ Aii ^ thyllrjCl catalyst carried out in the catfish Preparation of a polymer in which an ethylene-propylene random copolymer was block-copolymerized with a polypropylene IC chain (85 #, based on the block copolymer) Lifting product · The two components were kneaded together so that the amount of copolymer 3% by weight, based on the resulting oil. Then the Hasse was granulated and then the Spritztlber » Train test as in Böißpiel 1 subject to bsachriebon.

For comparison purposes, the above-mentioned high-pressure polyethylene was kneaded with both iootactic polypropylene and with low-pressure polyethylene, xtnd tertiary ethyl n-propylene copolymer so that the last-mentioned Eeccandtaile each made up wt .- ^, based on the total weight of the mass. The hating thus obtained vnirden granulating 'c and then subjected to the spray-Ubersug tests as described in Example. 1 Furthermore, the elongation of the coatings, the elongation of the wire cores and the abrasion resistance of the overmolded DrEhta were tested as indicated above. The results are shown in Table IV.

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Table IV

Schaslzindex (g / 10 min.) inventive
according to in the comparative tests
high pressure polyethylene approved polymer Polyethylene tern * ires
Xthylsn-Pro- density Forasasse Polypropylene 0.35 0.31 pressure (kg / cm) 0.38 0.37 0.324 0.921 Roughness of the coated upper
area 0.921 0.922 384.0 455.0 CD Elongation of the spray coating (£) 380.0 457.0. 8.0 10.0 (_?
CD
CO Stretching of the metal core {&) ' 2.0 6.0 303.0 383.0 cn Abrasion resistance (at 50 ⁰ C) 400.0 ' 265.0 ■ · - - KJ Load 50 g 26.0 23.0 O
* -> ⁿ 75 g 98.0 144.0 * ' ^β 100 g 107.0 59.0 61.0 28.0 37.0 20.0 31.0 9.0 15.0 9.0

3D 2.

CT) CO cn cn

Table IV shows that the results of the spray draw tests on the masses, in which in each case either polypropylene, low pressure polylitiiylen or ternary ethylene-propylene copolytiiar had been incorporated, essential ßchlischtora smooth the Excessive obscuration results in the masses of the invention. The table also shows that the reference weights The polypropylene and tern'dros Kthylen-Propylon-Copolymer require higher pressures than those according to the invention Porm masses. It is also clearly seen that in comparison to the invention pomimasses show the usual hates poorer elongation of the coatings and the wire seals and with regard to their processing bargain on high-cost mazohincn Have disadvantages.

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Claims (6)

Claims 1. Polymer-Pormmasse based on high pressure polyethylene, thereby characterized in that it consists essentially of (1) 70 to 99.5 weight percent of a high pressure polyethylene having a density of 0.9 ^ 0 or less and (2) 0.5 to 30 wt .- * of (a) a substantially amorphous polypropylene which is considered to be a sparingly soluble Polymerization by-product in the production of crystalline polypropylene using one made from a titanium halide and a catalyst consisting of an aluminum alkyl and preferably in n-heptane as a polymerization solvent, (b) an essentially amorphous propylene-ethylene copolymer, which is a sparingly soluble polymerization by-product in the Production of crystalline propylene-ethylene copolymer or crystalline propylene-ethylene block copolymer, essentially made of propylene using one made of a titanium halide and a catalyst consisting of an aluminum alkyl and preferably obtained in n-heptane as the polymerization medium, or (c) Mixture of such a substantially amorphous polypropylene with such a substantially amorphous propylene-xethylene copolymer. 2. Molding composition according to claim 1, characterized in that the proportion of the substantially amorphous polypropylene, the substantially amorphous propylene copolymer or the mixture of these two substances is 1 to 10 wt. 3. Molding composition according to claim 1. or 2, characterized in that it contains such a substantially amorphous propylene-ethylene copolymer which has an ethylene content of 20 wt. Jf or less, a viscosity number Ct) J in tetralin 135 ° C from 0.2 to 2.8 and a crystallinity determined by means of conventional X-ray analysis of 35% by weight or less / 4. Molding composition according to claim 1 or 2, characterized in that it contains such a substantially amorphous polypropylene which in tetralin at 135 ° C has a viscosity number &) 7 of 0.2 to 0.6 and one by means of conventional X-ray analysis found to have a crystallinity of 35 Ji by weight or less. 009851/2000 BATH ORIGINAL 5. Process for the production of a polymer mold according to Claim 1 to 4, characterized in that (1) 70 to 99 »5 Gaw.-Ji of a high-back polyethylene having a density of 0.9 -! - O or less and (2) 0.5 to 50 (S3W. ~ # Öines (a) Essentially amorphous polypropylene, which is considered a moderate soluble polymerization woven fabric in the manufacture of crystalline polypropylene using one of one Titanium halide and an aluminum alkyl toostehandcn catalyst is obtained, (b) essentially amorphous propylene-ethylene copolymer, that as a sparingly soluble polymerization Hoban product when listening to crystalline propyl-n-Ethyien-CopoljTuer or crystalline propylene-ethylene block copolymer, essentially made of propylene, using one of one Titanium halide and an aluminum alloy consisting of a catalyst is obtained, or (c) a mixture of such essentially amorphous polypropylene with such an essentially amorphous one Propylene-ethylene coptilofiQsr kneaded. 6. Electric wire, characterized in that it is connected to a Coating of (1) 70 to 99 * 5% by weight of a high pressure polyethylene with a density of 0.94-0 or less and (2) 0.5 to JO % By weight of a (a) substantially amorphous polypropylene which as a sparingly soluble polymorization byproduct in the Manufacture of crystalline polypropylene using one composed of a titanium halide and an aluminum alkyl Catalyst available, (b) essentially amorphous polypropylene-ethylene copolymer, that as a sparingly soluble polyrolyzate by-product in the production of crystalline propylene-ethylene copolymer or crystalline propylene-ethylene block copolymer, consisting essentially of propylene using one of a titanium halide and an aluminum alkyl existing catalyst is obtained, or (c) mixture of such a substantially amorphous polypropylene and a such a substantially amorphous propylene-ethylene copolymer is provided. 009851/2000 B ^AD 0 ^ftiGlNAL 7 * Method of coating an electric wire with a Polyraer-Fonranace, characterized in that one such « Polymer molding compound used, which consists essentially of (1) 70 to 99.5 wt. «# Of a high pressure polyethylene with a Density of 0.9 ^ 0 or less and (2) 0.5 to 30 wt. # Of one (a) essentially amorphous polypropylene, which is considered to be a moderate soluble polymerization by-product in the production of crystalline polypropylene using one of a .Titanium halide and an aluminum alkyl existing catalyst is obtained, (b) the essentially amorphous propylene-ethylene copolymer which is a sparingly soluble polymer isolone by-product in the production of crystalline propylene-ethylene copolyraer or crystalline propylene-ethylene block copolymer consisting essentially of propylene using one of a Titanium halide and an aluminum alkyl existing catalyst is obtained, or (c) Oemlsches from such an essentially amorphous polypropylene and a solo, essentially amorphous propylene-ethylene copolymer. 009851/2000 BAD